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Silicate ester flame-retardant plasticizer and preparation method thereof

A technology of flame retardant plasticizer and silicate, applied in the field of flame retardant plasticizer, can solve the problems of large investment and limited development, and achieve the effects of good compatibility, environmental protection and good application prospects.

Inactive Publication Date: 2013-04-03
寇洪燕
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the production of one ton of polysilicon will produce 15-20 tons of by-product silicon tetrachloride, and the treatment of silicon tetrachloride limits the development of the entire industry
At present, the successful method of treating silicon tetrachloride is to convert silicon tetrachloride into trichlorosilane, the raw material of polysilicon, but the investment is huge, and most polysilicon enterprises are unable to do what they want under the fierce market competition conditions.

Method used

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  • Silicate ester flame-retardant plasticizer and preparation method thereof
  • Silicate ester flame-retardant plasticizer and preparation method thereof
  • Silicate ester flame-retardant plasticizer and preparation method thereof

Examples

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Effect test

preparation example 1

[0024] Preparation Example 1 In a 150ml four-neck flask equipped with a stirrer, a thermometer and a high-efficiency reflux condenser, pass through nitrogen protection, add 0.1mol silicon tetrachloride, and start dropping 0.1mol methanol under the liquid surface at 20°C to react and release hydrogen chloride. After the hydrogen chloride is released, install an extremely flexible and expandable soft sealing sleeve on the mouth of the condenser, stir, and start to introduce 0.4mol ethylene oxide under the liquid surface at 20°C, cool in an ice-water bath, and control the temperature at the rate of introduction. After passing through, keep the temperature at about 30°C for another 2 hours, and then raise the temperature to 40°C for half an hour. Heat and reduce pressure to distill off excess reactants and a small amount of by-product chloroethanol and recycle them, and filter to obtain tris(chloroethyl)methyl silicate with a yield of 98%, a decomposition temperature of 224±5°C, an...

preparation example 2

[0025] Preparation Example 2 In a 150ml four-necked flask equipped with a stirrer, a thermometer and a high-efficiency reflux condenser, pass through nitrogen protection, add 0.1mol silicon tetrachloride, and start dropping 0.1mol methanol under the liquid surface at 20°C to react and release hydrogen chloride. After the hydrogen chloride is released, install an extremely flexible and expandable soft sealing sleeve on the mouth of the condenser, stir, and start to introduce 0.4mol of ethylene oxide under the liquid surface at 20°C, cool in an ice-water bath, and control the temperature at the rate of introduction , After passing through, maintain the temperature at about 20°C and react for another 2 hours. Heat and reduce pressure to distill off excess reactants and a small amount of by-product chloroethanol and recycle them, and filter to obtain tris(chloroethyl)methyl silicate. The yield is 96%, and the decomposition temperature is 224±5°C. The point (open cup) is 198±5°C, t...

preparation example 3

[0026] Preparation Example 3 In a 150ml four-neck flask equipped with a stirrer, a thermometer and a high-efficiency reflux condenser, pass through nitrogen protection, add 0.1mol silicon tetrachloride, and start dropping 0.1mol methanol under the liquid surface at 20°C to react and release hydrogen chloride. After the hydrogen chloride has been discharged, install a soft sealing sleeve that can be extremely stretched and expanded on the mouth of the condenser, stir, and start adding 0.3mol propylene oxide under the liquid surface at 20°C (gradually increase the temperature as the reaction progresses), cool in an ice-water bath, and The dropping speed controls the temperature, maintains the temperature at about 40°C and reacts for 6 hours, distills off the excess reactant and a small amount of by-product chloropropanol under reduced pressure and recycles it for use, and then filters it to obtain tris(chloropropyl)methyl silicate. Its yield is 95%, its decomposition temperature ...

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Abstract

The invention relates to a silicate ester flame-retardant plasticizer and a preparation method thereof. The structure of the compound is shown as the formula in the specifications, wherein n is more than or equal to 1 and less than or equal to 2; R is straight chain or branched chain alkyl with 1 to 12 carbon atoms; R' is hydrogen or methyl; and R'' is hydrogen, methyl or chloromethyl. The preparation method comprises the following steps of: under the protection of nitrogen, reacting silicon tetrachloride with alcohol according to a certain molar ratio to generate chlorine hydride; and then reacting the chlorine hydride with alkylene oxide according to a certain molar ratio to obtain a target product, or changing the material adding sequence to obtain the target product. The compound has stable physical and chemical properties, high flame-retardant performance, high plasticity and a simple process, and is easy to produce on a large scale.

Description

technical field [0001] The invention relates to a silicate flame-retardant plasticizer and a preparation method thereof, in particular to a silicate flame-retardant plasticizer prepared from silicon tetrachloride, alcohol and alkylene oxide as raw materials and a preparation method thereof. The compound is a silicon-halogen synergistic flame-retardant plasticizer, and can be used as a flame-retardant plasticizer for polyvinyl chloride, polyester, polyurethane, epoxy resin, glass fiber reinforced plastic resin, and coatings. Background technique [0002] At present, my country's solar-grade polysilicon industry (photovoltaic industry) has developed rapidly and has received widespread attention from all walks of life. However, the production of one ton of polysilicon will produce 15-20 tons of by-product silicon tetrachloride, and the treatment of silicon tetrachloride limits the development of the entire industry. At present, the successful treatment method of silicon tetrac...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K5/5415C07F7/04C08L27/06C08L67/00C08L75/04C08L63/00C09D7/12
Inventor 王彦林刁建高王乐然
Owner 寇洪燕
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